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WORLD INTELLECTUAL PROPERTY ORGANIZATION
International Bureau

PCX

INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT)

(51) International Patent Classification ^ :
A23L 2/44, 2/52

(11) International Publication Number: WO 96/26648

(43) International Publication Date: 6 September 1996 (06.09.96)

(21) International Application Number: PCT/US96/0164S

(22) International FUing Date: 6 February 1996 (06.02.96)

(30) Priority Data:

08/395,740

28 February 1995 (28.02.95)

(71) AppUcant: THE PROCTER & GAMBLE COMPANY

[US/US]; One Procter & Gamble Plaza, Cincinnati, OH
45202 (US).

(72) Inventors: SMITH, James, Arthur; 580 Belle Meade Farm

Drive, Loveland, OH 45140 (US). GRAUMLICH. Thomas.
Ray; 2703 North Dearborn Road, West Harrison, IN
47060 (US). SABIN, Robert, Phillip; 831 Dunore Road.
Cincinnati, OH 45220 (US). VIGAR, Judith, Wells; 7337
Woodcroft Drive, Cincinnati, OH 45230 (US).

(74) Agents: REED, T., David et al.; The Procter & Gamble
Company, 5299 Spring Grove Avenue, Cincinnati, OH
45217 (US).

(81) Designated States: AL, AM, AT, AU, AZ, BB, BG, BR, BY,
CA, CH, CN, CZ, DE, DK, EE, ES, FI, GB, GE, HU, IS,
JP, KE, KG, ICP, KR, KZ, LK, LR, LS, LT, LU, LV, MD,
MG, MK, MN, MW, MX. NO, NZ, PL, PT, RO, RU, SD,
SE, SG, SI, SK, TJ, TM, TR, TT, UA. UG, UZ, VN, ARIPO
patent (KE, LS, MW, SD, SZ, UG), Eurasian patent (AZ,
BY, KG. ICZ, RU, TJ. TM). European patent (AT, BE, CH,
DE, DK, ES, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE),
OAPI patent (BF, BJ, CF, CG, CI, CM, GA. GN, ML, MR,
NE, SN, TD, TG).

Published

With international search report.

Before the expiration of the time limit for amending the
claims and to be republished in the event of the receipt of
amendments.

(54) TiUe: PREPARATION OF NONCARBONATED BEVERAGE PRODUCTS HAVING SUPERIOR MICROBIAL STABILITY

(57) Abstract

Disclosed are noncarbonated beverage products with improved microbial stability, and processes for preparing them. The
noncarbonated beverage products have a pH of between 2.5 and 4.5 and comprise from about 300 ppm to about 3000 ppm of a polyphosphate
having an average chain length ranging from about 17 to about 60; from about 100 ppm to about 1(X)0 ppm of a preservative selected
from the group consisting of sorbic acid, benzoic acid, alkali metal salts thereof and mixtures thereof; from about 0.1 % to about 40 %
by weight of fruit juice; and from about 80 % to about 99 % by weigth of added water, wherein the added water contains from 61 ppm
to about 220 ppm of hardness. These noncarbonated beverage products can be stored at ambient temperatures for at least about 28 days
without substantial microbial proliferation therein after exposure to beverage spoilage organisms.

FOR THE PURPOSES OF INFORMATION ONLY

Codes used to identify States party to the PCT on the front pages of pamphlets publishing international
applications under the PCT.

Annenia

United Kingdom

Malawi

Austria

Georgia

Mexico

Australia

Guinea

Niger

Baitndos

Greece

Netherlands

Belgium

Hungary

Norway

Burkina Paso

Ireland

New Zealand

Bulgaria

Italy

Poland

Benin

Japan

Portugal

Brazil

Kenya

Romania

Belarus

Kyrgystan

Russian Federation

Canada

Democratic People's Republic

Sudan

Central African Republic

of Korea

Sweden

Congo

Republic of Korea

Singapore

Switzerland

Kazakhstan

Slovenia

C8«e d'lvoire

Liechtenstein

Slovakia

Cameroon

Sri Lanka

Senegal

China

Liberia

Swaziland

Czechoslovakia

Lithuania

Chad

Czech Republic

Luxembourg

Togo

Germany

Latvia

Tajikistan

Denmark

Monaco

Trinidad and Tobago

Estonia

Republic of Moldova

Ukraine

Spain

Madagascar

Uganda

Finland

Mali

United States of America

France

Mongolia

Uzbekistan

Gabon

Mauritania

Viet Nam

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PREPARATION OF NONCARBONATED BEVERAGE PRODUCTS HAVING

SUPERIOR MICROBIAL STABILITY
FIELD OF THE INVENTION

The present invention relates to noncaibonated beverage products having
superior microbial stability. Such stability is provided primarily by a novel combination
within the beverage products of sodium polyphosphates having a particular average
s chain length, a preservative and water of a specified hardness.

BACKGROUND OF THE INVENTION

Controlling microbial growth in noncarfoonated dilute juice beverages is an
ongoing concern among beverage manufacturers. Such beverage products, when

10 exposed to food spoilage microorganisms, provide an excellent environment for rapid
microbial growth. Such exposure can, and infrequently does, result from accidental
inoculation of the beverage products during manufacturing or packaging. Food
spoilage microorganisms can then rapidly proliferate by feeding on nutrients provided
by the fruit juice component of the noncarbonated dilute juice beverages.

15 Of course, microbial proliferation in noncarbonated dilute juice beverages will

not occur without the requisite product exposure to yeast or bacteria. Manufacturing
and packaging operations directed to the prevention of such exposure is preferred, but
provisions are often made for any infrequent accidental exposure to the isolated
beverage product. Such provisions are directed to limiting or preventing subsequent

20 microbial proliferation to thus limit or prevent food spoilage.

Microbial stability of dilute juice beverage products can be provided to some
extent by heat pasteurizing during packaging (hot packing) or by packaging under
completely aseptic conditions (aseptic packaging). Hot packing involves
pasteurization of the beverage and its container such that the resulting sealed beverage

25 product contains no food spoilage microorganism. Likewise, aseptic processing and
packaging of a pasteurized beverage will produce a beverage product completely free
of food spoilage microorganisms. Accordingly, these beverage products are extremely
shelf stable since there are assuredly no food spoilage microorganisms therein to feed
on the beverage nutrients and rapidly proliferate.

30 Aseptic packaging methods, however, are often unsuitable for manufacturing

beverages products packaged in certain beverage containers, e.g., rigid containers such
as glass, plastic and cans. An aseptic or sterile environment is difficult to maintain
during aseptic packaging operations. Frequent cleaning of the packaging line is
necessary which is time consuming and expensive.

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Hot packing methods are likewise unsuitable for manufacturing certain types of
beverage products. This well known method involves heat pasteurization of the juice
beverage during packaging at temperatures of between about 85°-105°C. This method
is commonly utilized in the manufacture of canned or bottled (glass) beverages.
5 However, not all beverage containers can withstand heat-pasteurization during
packaging. For example, flexible containers made from high density polyethylene,
which have become more popular with consumers, should not be subjected to the
pasteurization temperatures utilized during hot packing operations.

Preservatives have been used in noncarbonated dilute juice beverages to

10 provide some degree of microbial inhibition. Preservatives commonly used in beverage
products include, for example, sorbates, benzoates, organic acids, and combinations
thereof However, such preservatives often contribute an oflf-flavor to the beverage
products when used at the levels necessary to inhibit subsequent microbial proliferation
during storage. Moreover, when used at concentrations suflBciently low to avoid oflf-

15 flavor development, such preservatives have heretofore been unable to effectively
inhibit the growth of many preservative resistant spoilage microorganisms.

Accordingly, most noncarbonated dilute juice beverages are hot packed in cans
or glass bottles or aseptically packaged.

The foregoing considerations involving the effective inhibition of subsequent

20 microbial proliferation in noncarbonated dilute juice beverage products indicates that
there is a continuing need to identify noncarbonated dilute juice beverage products that
can be manufactured Avithout the use of hot packing or aseptic packing operations, and
that are shelf stable for a reasonable amount of time without the use of excessive
concentrations of preservatives. It has previously been discovered that certain chilled

25 noncarbonated dilute juice beverage products could be maintained at ambient
temperatures for at least about 10 days, preferably for at least about 20 days, without
substantial microbial proliferation therein.

Such chilled noncarbonated beverage products include from about 400 ppm to
about 1000 ppm of a preservative selected from the group consisting of sort^ic acid,

30 benzoic acid, alkali metal salts thereof and mixtures thereof; from about 0. 1% to about
10% by weight of fruit juice; and from about 900 ppm to about 3000 ppm of a
polyphosphate having the formula

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M --0— P— 0-- M

where n averages from about 3 to about 100, preferably from about 13 to about 16.
and each M is independently selected from the group of sodium and potassium atoms.
The noncaibonated beverage products further comprise from about 80% to about 99%
added water by weight of the beverage products, wherein the added water contains
from 0 ppm to about 60 ppm of hardness, and preferably from 0 ppm to about 300
ppm of alkalinity. The noncarbonated beverage products have a pH of from about 2.5
to about 4.5 and an ambient display time of at least about 10 days.

Unfortunately, these chilled noncarbonated beverages do not necessarily
provide microbial stability at ambient temperature when the added water component of
these beverages has a hardness of more than about 60 ppm. Since water supplies used
for preparing these noncarbonated beverages frequently have a hardness of well above
60 ppm, it is often necessary to treat or "soften" the water before it can be
incorporated into the beverages hereinbefore described.

Conventional methods for softening water can be very expensive. Moreover, it
is not always possible or convenient to soften water to less than about 60 ppm using
conventional techniques. For example, one conventional method for softening water
involves treating the water with Ca(OH)2. This well known method is most suitable
and economical for water having an initial hardness of 100 to 150 ppm as calcium
carbonate. However, it is not uncommon for water sources to have a hardness in
excess of 150 ppm. Another conventional method for softening water involves ion-
exchange operations. This method, however, is preferably used to soften water having
an initial hardness of 50-100 ppm.

Due to the costs associated with softening of water and to limitations in the
methods themselves, it is an object of the present invention to provide noncarbonated
beverages having microbial stability at least equal to that of previous noncarbonated
beverages, but wherein the added water component can comprise water having a
hardness in excess of 60 ppm to avoid the cost and difficulties associated with having
to soften the water to a level below 60 ppm first. It is a fiirther object of the present
invention to increase the microbial stability of the beverages of the present invention
compared to prior beverages.

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SUMMARY OF THE INVENTION

The present invention is directed to noncarbonated dilute juice beverage
products having superior microbial stability. These beverages, after an initial
contamination level of 10 cfu/ml of spoilage microorganisms, exhibit less than a 100
fold increase in the level of microorganisms when stored at 73 "F for at least 28 days.
The beverage products do not require hot packing, aseptic packing or the
incorporation of excessive amounts of preservatives to provide the requisite inhibition
of microbial proliferation during storage.

Essential elements of the noncarbonated beverage products of the present
invention include 1) a preservative system comprising a) from about 100 ppm to about
1000 ppm of a preservative selected from the group consisting of sorbic acid, benzoic
acid, alkali metal salts thereof and mixtures thereof, and b) from about 300 ppm to
about 3000 ppm of a sodium polyphosphate having the formula

Na--0— P— O-

where n averages from about 17 to about 60; 2) from about 0. 1% to about 40% by
weight of a fruit juice and/or from about 0 to about 0.25% of a tea solids component;
and 3) from about 80% to about 99% added water by weight of the beverage products.
The added water contains from about 6 1 ppm to about 220 ppm of hardness. The
noncarbonated beverage products have a pH of from about 2 .5 to about 4.5.

DETAILED DESCRIPTION OF THE INVENTION
As used herein, "microbial proliferation" means a 100 fold increase or greater
in the number of beverage spoilage microorganisms in a noncarbonated beverage
product after an initial contamination level of about 10 cfii/ml. Beverage products
described as "microbially stable" exhibit less than a 100 fold increase in the level of
microorganisms when stored at 73 "F for at least 28 days, following an initial
contamination level of 10 cfii/ml of spoilage microorganisms. Beverages described as
"microbially unstable" exhibit more than a 100 fold increase in the level of
microorganisms when stored at 73 "F for 28 days, following an initial contamination
level of 10 cfli/ml of spoilage microorganisms.

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As used herein, the term "noncarbonated beverage products" refers to beverage
products having less than 1 volume of carbonation.

As used herein, the term "comprising" means various components can be
conjointly employed in the preparation of the noncarbonated beverage products of the
present invention.

All weights, parts and percentages used herein are based on weight unless
otherwise specified.

Preparation of the noncarbonated beverage products of the present invention is
described in detail as follows.

The Preservative System

The noncarbonated beverage products of the present invention comprise a
preservative system containing a preservative and a food grade polyphosphate. The
preservative system is described in detail as follows.

A. The Preservative

Specifically, the beverage products herein comprise fi'om about 100 ppm to
about 1000 ppm, preferably fi'om about 200 ppm to about 650 ppm, more preferably
fi'om about 400 ppm to about 650 ppm, of a preservative selected fi'om the group
consisting of sorbic acid, benzoic acid, alkali metal salts thereof, and mixtures thereof
The preservative is preferably selected fi'om the group consisting of sorbic acid,
potassium sorbate, sodium sorbate and mixtures thereof Most preferred is potassium
sorbate.

B. The Food Grade Polyphosphate

The noncarbonated beverage products further comprise a food grade sodium
polyphosphate for use in combination with the preservative. Specifically, the beverage
products comprise firom about 300 ppm to about 3000 ppm, preferably fi'om about 500
ppm to about 3000 ppm, more preferably fi'om about 900 to about 3000 ppm, most
preferably fi'om about 1000 ppm to about 1500 ppm, of a sodium polyphosphate
characterized by the following structure:

Na +0— P— O+Na

where n averages fi'om about 17 to about 60, preferably fi'om about 20 to about 30.
Especially preferred is sodium polyphosphate, a straight chain sodium polyphosphate

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where n averages about 21 .

It has found that these straight chain polymeric phosphates exhibit better
antimicrobial activity in the noncarbonated beverage products of the present invention
than other food grade phosphates. Well-known food grade phosphates include, for
5 example, orthophosphate, cyclic polyphosphates, monobasic calcium phosphate,
dipotassium phosphate, disodium phosphate, sodium phosphate, sodium
pyrophosphate, sodium metaphosphate and tetrasodium pyrophosphate.

The polyphosphates for use in the noncarbonated beverage products herein and
the selected preservatives also for use in the beverage product herein act
10 synergistically, or at least additivity, to inhibit microbiological growth in the beverage
products of the present invention. This combination in the beverage products herein is
particularly effective in inhibiting yeast, including preservative resistant
Zygosaccharomyces bailii, and acid tolerant preservative resistant bacteria.

The use of sorbates, benzoates and mixtures thereof as preservatives in
15 beverage products is well known, as is the mechanism by which such preservatives
inhibit microbial groAvth in food products generally. Sorbates and benzoates are
described, for example, by Davidson and Branen, Antimicrobials in Foods . Marcel
Dekker, Inc., pp. 11-94 (2nd ed. 1993), which description is incorporated herein by
reference.

20 The use of straight chain polyphosphates, alone or in combination with

preservatives, to inhibit microbial growth in food products is also well known.
Polyphosphates are described, for example, in Handbook of Food Additives. CRC
Press, pp. 643-780 (2nd ed.l972), which description is incorporated herein by
reference. Moreover, the synergistic or additive antimicrobial effect from phosphates

25 combined with a preservative (e.g., sorbates, benzoates, organic acids) in food
products is disclosed in U.S. Patent 3,404,987 to Kooistra et al.

Although the use of the above-described polyphosphates and preservatives,
alone or in combination, do provide some degree of antimicrobial activity in the
beverage products, the novel beverage product of this invention described hereinafter

30 shows outstanding antimicrobial activity against microorganisms commonly associated
with the spoilage of beverage products, especially preservative resistant spoilage
microorganisms.

Moreover, it has also been found that the particular straight chain polymeric
sodium phosphates described herein (e.g., those having an average chain length
35 ranging from about 1 7 to about 60), provide superior microbial stability to beverages
containing them compared to straight chain polymeric phosphates having an average
chain length of other than from about 17 to about 60, especially when the water

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hardness of the added water component of the beverages (hereinafter described) ranges
from 61 ppm to about 220 ppm. In particular, the noncarbonated beverages herein,
which contain straight chain polymeric sodium phosphates having an average chain
length ranging from about 17 to about 30, will exhibit less than a 100 fold increase in
5 the level of microorganisnis when stored at 73"? for at least 28 days, after an initial
contamination level of 10 cfii/ml of spoilage microorganisms. Preferably, the
beverages herein will exhibit less than a 100 fold increase in the level of
microorganisms when stored at 73°F for at least 60 days, more preferably at least 100
days, after an initial contamination level of 10 cfii/ml of spoilage microorganisms. In

10 general, the lower the water hardness of the added water, the longer the beverage will
remain microbially stable.

It is believed that the improved microbial stability of the noncarbonated
beverages herein which contain straight chain polymeric sodium phosphates having an
average chain length of from about 17 to about 60 can be attributed to the particular

15 characteristics of the straight chain polymeric sodium phosphates employed. It is
believed that, upon hydrolysis, straight chain polymeric sodium phosphates having an
average chain length of from about 17 to about 60 break down to straight chain
polymeric sodium phosphates that are still effective in providing microbial stability to
the beverages containing them. By contrast, straight chain polymeric phosphates

20 having an average chain length of less than about 21 will hydrolyze into straight chain
polymeric phosphates which are not effective in providing microbial stability to the
beverages containing them. Straight chain polymeric phosphates having an average
chain length of greater than about 60 are not necessarily soluble in the beverage
products described herein.

25 Another advantage of the straight chain polymeric sodium phosphates of the

present invention is that they can provide microbial stability to the beverages herein
even when the added water component of the beverages comprises moderately hard to
hard water. Thus, there is frequently no need to soften the water before it is
incorporated into the b^erage.

30 The Added Water Component

The noncarbonated beverages herein also comprise an added water component.
For purposes of defining the beverage products herein, the added water component
does not include water incidentally added to the beverage product via other added
materials such as, for example, the fruit juice component. The beverage products of
35 the present invention typically comprise from about 80% to about 99% by weight of
water, more typically from about 85% to about 93% by weight of water.

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The term "hardness" as used herein refers to the presence of calcium and
magnesium cations in water, generally. For purposes of the present invention,
hardness of the added water component is calculated according to Association of
Official Analytical Chemists (AOAC) standards set forth in Official Methods of
5 Analysis, published by the AOAC, Arlington, Virginia, pp. 627-628 (14th ed. 1984),
which is incorporated herein by reference. Under AOAC standards, hardness is the
sum of CaC03 equivalents (mg/L) in water, which sum is obtained by multiplying the
concentrations (mg/L) found of the following cations in the water by the factors.

Table 1

Cation

Factor

2.497

4.116

1.142

1.792

5.564

1.531

1.822

Compounds that impart hardness to water are primarily magnesium and
calcium carbonates, bicarbonates, sulfates, chlorides and nitrates, although other
compounds which can contribute polyvalent cations to water can also impart hardness.
Water based on hardness is normally classified as soft (0-60 ppm), moderately hard

15 (6 1 - 1 20 ppm), hard ( 1 2 1 - 1 80 ppm) and very hard (over 1 80 ppm).

As stated hereinbefore, the antimicrobial efifects of the beverage products of the
present invention are evident at water hardness levels above about 60 ppm. In fact, the
antimicrobial effects of the noncarbonated beverages of the present invention are
evident when the hardness of the added water component of the beverages ranges from

20 61 to about 220 ppm. Preferably, the hardness of the added water component ranges
from 61 to about 200 ppm, more preferably from 61 to about 180 ppm, and most
preferably from 61 ppm to about 140 ppm.

The Fruit Juice and/or Tea Solid Component

In one embodiment of the present invention, the beverage products contain
25 fruit juice, which can provide flavor and nutrition. However, it is the fruit juice that
also provides an excellent medium on which beverage spoilage microorganisms can
feed and rapidly proliferate. It is therefore this fruit juice component of the
noncarbonated beverage product herein that necessitates the use of the preservative

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system and water quality controls described hereinbefore.

Specifically, the noncarbonated beverage product of the present invention can
comprise from 0.1% to about 40%, preferably from about 0.1% to about 20%, more
preferably fi-om about 0.1% to about 15%, and most preferably fi-om about 3% to
5 about 10%, by weight of a fruit juice (weight percentage based on single strength 2-16
° Brix fruit juice). The fiuit juice can be incorporated into the beverage product as a
puree, comminute or as a single strength or concentrated juice. Especially preferred is
the incorporation of the fruit juice as a concentrate with a solid content (primarily as
sugar solids) of between about 20° and 80° Brix.

10 Subsequent microbial proliferation in the noncarbonated beverage product

herein will not necessarily be effectively inhibited during storage if fruit juice
concentrations exceed about 40% by weight of the beverage products. At fruit juice
concentrations less than about 0.1% by weight of the beverage product, the need for
stringent antimicrobial systems is less. Even within the fruit juice concentrations of the

15 beverage product herein (between about 0.1% and about 40%), microbial stability will
increase with decreased percentages of fruit juice in the beverage product. Variations
in the concentration of preservative and polyphosphate within the ranges described
hereinbefore can also impact microbial stability. Nonetheless, so long as the
concentration of fhiit juice, preservative, polyphosphate, and water hardness are within

20 the ranges recited herein for the beverage products, the beverages herein will be
microbially stable.

The fruit juice in the noncarbonated beverage products can be any citrus juice,
non-citrus juice, or mixture thereof, which are known for use in beverage products
Examples of such fioiit juices include, but are not limited to, non-citrus juices such as

25 apple juice, grape juice, pear juice, nectarine juice, currant juice, raspberry juice,
gooseberry juice, blackberry juice, blueberry juice, strawberry juice, custard-apple
juice, pomegranate juice, guava juice, kiwi juice, mango juice, papaya juice,
watermelon juice, cantaloupe juice, cherry juice, cranberry juice, pineapple juice, peach
juice, apricot juice, plum juice and mixtures thereof, and citrus juices such as orange

30 juice, lemon juice, lime juice, grapefruit juice, tangerine juice and mixtures thereof
Other fruit juices, and nonfioiit juices such as vegetable or botanical juices, can be used
as the juice component of the noncarbonated beverage products of the present
invention.

The noncarbonated beverage products herein can also comprise tea solids. The
35 tea solids can be incorporated into the beverage product in addition to, or in place of,
the fruit juice component described hereinbefore.

Specifically, the noncarbonated beverage products can comprise from 0 to

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about 0.25%, preferably from about 0.02% to about 0.25%, more preferably from
about 0.7% to about 0.15%, by weight of tea solids. The term "tea solids" as used
herein means solids extracted from tea materials including those materials obtained
from the genus Camellia including C. sinensis and C. assaimica, for instance, freshly
5 gathered tea leaves, fresh green tea leaves that are dried immediately after gathering,
fresh green tea leaves that have been heat treated before drying to inactivate any
enzymes present, unfermented tea, instant green tea and partially fermented tea leaves.
Green tea materials are tea leaves, tea plant stems and other plant materials which are
related and which have not undergone substantial fermentation to create black teas.

10 Members of the genus Phyllanthus, catechu gambir and Uncaria family of tea plants
can also be used. Mixtures of unfermented and partially fermented teas can be used.

Tea solids for use in the noncarbonated beverage products herein can be
obtained by known and conventional tea solid extraction methods. Tea solids so
obtained will typically comprise caffeine, theobromine, proteins, amino acids, minerals

IS and carbohydrates.

Sweetener

The noncarbonated beverage products of the present invention can, and
typically will, contain an artificial or natural, caloric or noncaloric, sweetener.
Preferred are carbohydrate sweeteners, more preferably mono- and or di-saccharide
20 sugars.

Specifically, the noncarbonated beverage products will typically comprise from
about 0.1% to about 20%, more preferably from about 6% to about 14%, sugar solids
by weight of the beverage products. Suitable sweetener sugars include maltose,
sucrose, glucose, fhiaose, invert sugars and mixtures thereof These sugars can be

25 incorporated into the beverage products in solid or liquid form but are typically, and
preferably, incorporated as a syrup, more preferably as a concentrated syrup such as
high fructose com syrup. For purposes of preparing the beverage products of the
present invention, these optional sweeteners can be provided to some extent by other
components of the beverage products such as the fhiit juice component, optional

30 flavorants, and so forth.

Preferred carbohydrate sweeteners for use in the beverage products are
sucrose, fructose and mixtures thereof Fructose can be obtained or provided as liquid
fructose, high fructose com syrup, dry fructose or fiuctose syrup, but is preferably
provided as high fructose com syrup. High fructose com symp (HFCS) is

35 commercially available as HFCS-42, HFCS-55 and HFCS-90, which comprise 42%,
55% and 90%, respectively, by weight of the sugar solids therein as fructose.

Optional artificial or noncaloric sweeteners for use in the noncarbonated

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beverage product include, for example, saccharin, cyclamates, sucrose, acetosulfam, L-
aspartyl-L-phenylalanine lower alkyl ester sweeteners (e.g., aspartame), L-aspartyl-D-
alanine amides disclosed in U.S. Patent 4,411.925 to Brennan et al., L-aspartyl-D-
serine amides disclosed in U.S. Patent 4,399,163 to Brennan et al., L-aspartyl-L-l-
5 hydroxymethyl-alkaneamide sweeteners disclosed in U.S. Patent 4,338,346 to Brand,
L-aspartyl-l-hydroxyethylakaneamide sweeteners disclosed in U.S. Patent 4,423,029
to Riz2a, L-aspartyl-D-phenylglycine ester and amide sweeteners disclosed in European
Patent Application 168,112 to J. M. Janusz, pubUshed January 15, 1986, and the Uke.
A particularly preferred sweetener is aspartame.

10 Other Ingredients

The noncarbonated beverage products herein can further comprise any other
ingredient or ingredients typically used as optional beverage ingredients. Such optional
ingredients include flavorants, preservatives (e.g., organic acids), colorants and so
forth.

15 The noncarbonated beverage products can forther comprise from 0 to about

110% of the U.S. Recommended Daily Allowance (RDA) of vitamins and minerals,
provided that such vitamins and minerals do not substantiaUy reduce ambient display
times of the noncarbonated beverage products, and that such vitamins and minerals are
chemically and physicaUy compatible with the essential elements of the noncarbonated

JO beverage products. Especially preferred are vitamin A, provitamins thereof (e.g., beta
carotene), and ascorbic acid, although it is understood that other vitamins and minerals
can also be used.

It is well known that certain food grade polyphosphates, such as those
described herein, can help inhibit inactivation of the ascorbic acid while in the beverage

:5 product. It is also important to note that calcium, iron and magnesium fortification
should be avoided since these polyvalent cations can bind to and inactive the
polyphosphate component of the noncarbonated beverage products.

Gums, emulsifiers and oils can be included in the beverage products to affect
texture and opacity. Typical ingredients include guar gum, xanthan, alginates, mono-

0 and di-glycerides, lecithin, pectin, pulp, cottonseed oil, vegetable oU, food starches and
weighting oils/agents. Esters and other flavor and essence oils can also be
incorporated into the beverage products.

Acidity

The noncarbonated beverage products of the present invention have a pH of
5 from about 2.5 to about 4.5, preferably from about 2.7 to about 3.5, most preferably
from about 3.0 to about 3 .3. This pH range is typical for noncarbonated dilute juice

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beverage products. Beverage acidity can be adjusted to and maintained within the
requisite range by icnown and conventional methods, e.g., the use of food grade acid
bufifers. Typically, beverage acidity within the above recited ranges is a balance
between maximum acidity for microbial inhibition and optimum acidity for the desired
S beverage flavor and sourness impression. In general, the lower the acidity of the
beverage, the more effective the sodium polyphosphate will be at providing microbial
stability. Thus, the lower the acidity of the beverage, the less sodium polyphosphate
and/or preservative is required to provide microbial stability. Alternatively, when the
acidity of the beverage is low, the amount of juice in the beverage can be increased.

10 PreparHtion

The noncarbonated beverage products of the present invention can be prepared
by conventional methods for formulating noncarbonated dilute juice beverages. Such
conventional methods can involve hot packing or aseptic packaging operations,
although such operations are not necessary for achieving the extended ambient display

15 times described hereinbefore.

Methods for making dilute juice beverages, for example, are described in U.S.
Patent 4,737,375 to Nakel et al., which is incorporated herein by reference. Methods
for making beverage products are also described by Woodroof and Phillips, Beverag es:
Carbonated & Noncarbonated. AVI Publishing Co.(rev. ed. 1981); and by Thomer and

20 Herzberg, N on-alcoholic Food Service Beverage Handbook. AVI Publishing Co. (2nd
ed. 1978).

One method for preparing the beverage products herein involves making a
beverage concentrate, adding to it to a sugar syrup containing polyphosphate, and then
trimming the mixture with water, sugar syrup, and beverage concentrate to obtain the

25 requisite acidity and material composition. All added water used in such a preparation
must have, or be adjusted to, the requisite hardness. In such a method, the beverage
concentrate can be prepared by admixing to water (correct hardness) an acidulant
(e.g., citric acid), water soluble vitamins, flavorants including juice concentrate, and
preservative. An oil in water emulsion, which provides opacity and texture to the

30 beverage products, can be added to the concentrate. The sugar syrup for use in
preparing the beverage products is separately prepared by adding sugar syrup (e.g.,
high fiuctose com syrup) to water, and then adding ascorbic acid, polyphosphate and
thickening agents to the syrup. Additional preservative can be added to the resulting
sugar syrup. The sugar syrup and concentrate are combined to form a noncarbonated

35 beverage product. The noncarbonated beverage product can be trimmed with small
amounts of added water, sugar syrup and beverage concentrate to achieve the requisite
acidity and composition of the noncarbonated beverage product of the present

wo 96/26648

PCT/US96/01645

-13-

invention. It can then be pasteurized, packaged and stored. It is understood that other
methods, e.g., the methods described hereinafter in the EXAMPLES seaion, can be
used to prepare the noncarbonated beverage products herein

The key aspect of the process of the present invention is admixing the requisite
5 materials, in the requisite amounts, to achieve the noncarbonated beverage products of
the present invention. Other well known and conventional variations of the above
described beverage formulation technique can, therefore, be used to prepare the
noncarbonated beverage products herein.

Test Method: Microbial Stability

10 The term "microbial proliferation" as used herein means a 100 fold increase or

greater in the number of beverage spoilage microorganisms in a noncarbonated
beverage product after an initial inoculation level of about 10 cfli/ml. Beverage
products described as "microbially stable" exhibit less than a 100 fold increase in the
level of microorganisms when stored at 73°F for at least 28 days, following an initial

15 contamination level of 10 cfu/ml of spoilage microorganisms. Beverages described as
"microbially unstable" exhibit more than a 100 fold increase in the level of
microorganisms when stored at 73 for 28 days, following an initial contamination
level of 10 cfu/ml of spoilage microorganisms.

The microbial stability a noncarbonated beverage product can be determined by

20 the following method. Beverage products are inoculated with mixed groups of
preservative resistant yeast containing at least four separate yeast isolates, including
Zygosaccharomyces bailii, and with mixed groups of preservative resistant, acid
tolerant bacteria, including Acetobacter species. All yeast and bacteria utilized in the
inoculation are previously isolated fi'om preserved fruit juice beverages. Inoculated

25 beverage products are maintained at 20°C for at least 60 days and aerobic plate
cultures performed periodically. Aerobic plate counts of both yeast and bacteria
populations are performed as described in the Compendium of Methods for the
Microbiological Examinations of Foods, American Public Health Association,
Washington, D.C. (edited by C. Vanderzant and D.F. Splittstoesser), which description

30 is incorporated herein by reference. These plate counts are then used to identify the
degree of microbial proliferation in the inoculated beverage product.
Test Method; Average Chain Length of Sodium Polyphosphate
Reagents and Equipment:
Deuterium Oxide (D2O)

35 NMR tubes 5 mm OD, Wilmad Glass, 507PP

10 mm OD, Wilmad Glass, 513-5PP

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PCT/US96/01645

•14-

NMR tube pressure caps

Disposable transfer pipets
Probe for AC-300
Pyrex wool
Disposable wipers
Spinner Turbine

Spectrometer

5 mm OD, Wilmad Glass, 521
10 mm OD, Wilmad Glass, 521-C
Curtin Matheson, 355-123
5 or 10 mm
Coming Glass

Kimberly-Clark, Kim-Wipes
5 mm, Bruker
10 mm, Bruker

Bruker AC-300, equipped with 5 mm or 10 mm
probe

Procedure:

1. Dissolve about 100 mg of sample in deuterium oxide (D2O) to prepare a
solution having a concentration of about 12% by weight of sample. Warm

IS solution gently, if necessary, to aid in solute dissolution. Filter the solution

through compressed Pyrex wool, if necessary, to remove any solid particles.

2. Transfer the solution to a clean NMR tube, using a disposable pipet.

3. Place cap on NMR tube. Wipe all smudges and dust particles off the NMR
tube with a disposable wiper.

20 4. Prepare a barcode label including user's initials, spectrometer, microprogram

and sample solvent, and attach the label to the barcode label holder.

5. Place the barcode label holder in the NMR tube with lettering up and place
the spinner below the holder.

6. Position the sample using the depth gauge.

25 7. Place the sample tube/spinner/barcode holder assembly into the appropriate

chute on the spectometer sample changer.
S. The spectrum will be automatically obtained, processed and plotted, based on
the experiment and solvent information specified on the barcode label.
Spectrometer Parameters:
30 MicroproKram PHG

121.39 MHz
50 KHz
64K

2 usee = 45°

35 Pulse Recvcle 10.0 sec

Microprogram
Sweep Frequency
Sweep Width
Spectrum Size
Pulse Width
Pulse Recycle

Inverse gated broadband H-1 decoupling

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PCT/US96/01645

-15-

The average chain length of the sodium polyphosphate is calculated as follows:

Average chain length = ll ^'^^Srated Peak Area I ^ Imegrared Peak Area t\

\ Integrated Peak Area T /

5 Region T from -5 to -10 ppm contains peaks assigned to terminal phosphate units in
linear polyphosphates having a chain length of 2 or greater.

Region I from -18 to -24 ppm contains peaks assigned to internal phosphates. Cyclic
phosphates present as impurities in the samples also have peaks in Region I and are
10 included in the calculation.

The chemical shifts were referenced to external phosphoric acid.

EXAMPLES

The following includes specific embodiments of the noncarbonated beverage
15 products, and processes for making them, of the present invention. Ingredients for
each product are admixed in the order in which they appear. Sodium
hexametaphosphate for each product is admixed under high sheer mixing to insure
solubility. Ambient display time for each product is at least about 28 days. These
specific embodiments are illustrative of the invention and are not intended to be
20 limiting of it.

Embodiment 1

Ingredients

Added Water about 84%
hardness 140 ppm
25 Sodium hexametaphosphate (n= 22.76) ISOO ppm

Potassium sorbate 200 ppm
Fruit juice concentrate 1.75%

(as single strength juice 10%)
Citric acid about 0.24%
30 HFCS-55 about 13.5%

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PCT/US96/01645

-16-

Embodiment 2

Ingredients

Added Water about 98%
hardness 140 ppm
5 Sodium hexametaphosphate (n=23. 14) 1500 ppm

Potassium sorbate 200 ppm
Fruit Juice concentrates 1.75%

(as single strength juice 10%)
Citric acid about 0.24%
10 Aspartame about 500 ppm

Comparative Data

Noncarbonated beverage samples (A-C) are prepared and tested for microbial
stability according to the test method described hereinbefore in the Analytical Methods
section. Each sample contains 200 ppm sorbate and 98% by weight of added water

15 having a hardness of 140 ppm. Sample A contains 1500 ppm of sodium
hexametaphosphate with an average chain length of about 13. Sample B
(representative of the present invention) contains 1500 ppm of a sodium
hexametaphosphate with an average chain length of about 21. Each sample also
contains other minor ingredients which had substantially no effect on microbial

20 proliferation. Test results are summarized below.

LOG (cfu/ml)

Sample

0 days

29 days

58 days

99 days

1.10

1.33

4.10

5.2

1.03

2.58

2.57

2.40

Both samples are microbially stable after 29 days. However, after 58 days,
Sample A is no longer microbially stable, while Sample B remains microbially stable
even after 99 days.

25 [9994^rrMR
shw

wo 96/26648

PCTAJS96/01645

CLAIMS 17

1 Noncarbonated beverage products characterized by superior microbial stability,
comprising:

(a) from 100 ppm to 1000 ppm of a preservative selected from the group
consisting of sorbic acid, benzoic acid, alkali metal salts thereof and
mbctures thereof;

(b) from 0. 1 % to 40% by weight of fiuit juice;

Na--0— P— 0--Na

O
I

where n averages from 17 to 60; and

(d) from 80% to 99% by weight of added water having from 61 ppm to

220 ppm of hardness;
wherein the resulting noncarbonated beverage products have a pH of from 2.5
to 4.5 and wherein the beverage products, after an initial contamination level of
10 cili/ml of spoilage microorganisms, exhibit less than a 100 fold increase in
the level of microorganisms when stored at 23°C for at least 28 days.

2. A process for preparing noncarbonated beverage products characterized by
superior microbial stability, which process comprises admixing:

(a) from 100 ppm to 1000 ppm of a preservative selected from the group
consisting of sorbic acid, benzoic acid, alkali metal salts thereof and
mixtures thereof;

(b) from 0. 1% to 40% by weight of fruit juice;

wo 96/26648

PCT/US96/01645

Na--0 — P — 0--Na

where n averages from 17 to 60; and

(d) from 80% to 99% by weight added water having from 61 ppm to 220
ppm of hardness;

wherein the resulting noncarbonated beverage products have a pH of from 2.5
to 4.5 and wherein the beverage products, after an initial contamination level of
10 c£u/ml of spoilage microorganisms, exhibit less than a 100 fold increase in
the level of microorganisms when stored at 23*0 for at least 28 days.

3. The process of Claim 1 or 2 wherein from 0. 1% to 20% by weight of the fruit
juice is admixed into the noncarbonated beverage products.

4. Noncarbonated beverage products charaterized by improved microbial stability,
comprising:

(a) from 100 ppm to 1000 ppm of a preservative selected from the group
consisting of sorbic acid, benzoic acid, alkali metal salts thereof and
mixtures thereof;

(b) from 0.02% to 0.25% by weight of tea solids;

Na--0— P— 0--Na

where n averages from 1 7 to 60; and

(d) from 80% to 99% by weight added water having from 61 ppm to 220
ppm of hardness;

wherein the resulting noncarbonated beverage products have a pH of from 2.5 to 4.5
and wherein the beverage products, after an initial contamination level of 10 cfii/ml of

wo 96/26648

PCTAJS96/01645

spoilage microorganisms, exhibit less than a 100 fold increase in the level of
microorganisms when stored at 23 °C for at least 28 days.

5. The noncarbonated beverage products of Claim 1, 2, 3 and 4 wherein the
preservative is potassium sorbate and the sodium polyphosphate has an average chain
length ranging from 20 to 30.

6. The noncarbonated beverage products of Claim 5 wherein said beverage
products comprise from 1000 ppm to ISOO ppm of the sodium polyphosphate and
from 200 ppm to 650 ppm of the potassium sorbate.

7. The noncarbonated beverage products of Claim 6 wherein the added water
contains from 61 ppm to 180 ppm of hardness.

8. The noncarbonated beverage products of Claim 7 wherein the beverage
products have pH ranging from 3.0 to 3.3 and wherein, after an initial contamination
level of 10 cfu/ml of spoilage microorganisms, the beverages exhibit less than a 100
fold increase in the level of microorganisms when stored at 23°C for at least 60 days.

INTERNATIONAL SEARCH REPORT

'naaonal ApplicaQon No

PCT/US 95/G1645

A. CLASSIFICATION OF SUBJECT MATTER

IPC 6 A23L2/44

A23L2/52

According to IntemaBonal Patent Cla«ification (IPC) or to both national clasnfication and IPC

B. FIELDS SEARCHED

Minimum documentation searched (clarification system followed by classincation symbols)

IPC 6 A23L

OocumentaOon searched other than minimum documentation to the extent that such documents are included in the helds searched

Electronic data base consulted dunng the international search (name of data base and, where practical, search terms used)

C. DOCUMENTS CONSIDERED TO BE RELEVANT

Category * Citation of document, with mdicaoon. where appropriate, of the relevant passages

Relevant to claim No.

DE,A,17 92 760 (STAUFFER CHEMICAL CO) 30
May 1974

see page 1 - page 2

see page 16; examples 1-4

US, A, 3 681 091 (KOHL WILLIBALD F ET AL) 1
August 1972

see claim 12; examples 17,26

DE,A,16 42 141 (STAUFFER CHEMICAL CO.) 15
April 1971

see page 4, paragraph 2

US, A, 4 748 033 (SYFERT SCOTT W ET AL) 31
May 1988

see column 6, line 18 - line 19

see column 8, line 61 - column 9, line 6

-/--

1-8
1-8

1-8
1-8
1-8

Further documents are listed in the continuation ol box C.

Patent family members are listed in annex.

Special categories of cited documents :

'A' document dcrining the ];cncraJ sxatc ot the art which is not
considered to be ot particular relevance

'E' carher document but pubhshcd on or aticr the intcrnauonal
lilini^ date

L' document which may throw doubts on pnonty claim(s) or
which IS cited to estabhsh the publication date ot another
ctUQon or other spcaal reason |as spectlied)
*0* document referring to an oral disclosure, use, exhibition or
other means

' P" document published pnor to the intemaUonal fihng date but
later than the pnonty date claimed

T' later document published after the intemaQunal liling date
or pnoniy dale and not in conllict with the application hut
cited to understand the pnnciple or theory underlying the
mvenuon

X' document of parhcular relevance; the claimed invention
cannot he considered novel or cannot be con^dered to
involve an invenave step when the document is taken alone

Y' dtKumcnt of particular relevance; the claimed invcnUon
cannot he considered to involve an inventive step when the
document is combined with one or more other such docu-
ments, such combinahon being obvious to a person stalled
in the an.

' ^^ document member ol the same patent family

Date ol the actual completion ol the intcrnauonal search

31 May 1996

Date ol mailing of the international search report

0 'J. 07. 96

\ame and mailing address ol the ISA

European Patent Oilicc, P.B. iSlS PatenUaan :
NL - 2280 MV RijsOTik

Tel. ( - 31-^0) 34U-2l)4U. fx. 31 ept) nl.
Fax: ( - 31 ■70) 340-3016

Aulhonzed oKiccr

Bendl, E

Form PCT ISA2II) llecond I^ee^) (July 1992

page 1 of 2

INTERNATIONAL SEARCH REPORT

:mat]onal Application No

PCT/US 96/01645

C.(ConQnuaQan) DOCUMENTS CONSIDERED TO BE RELEVANT

Category ' Citauon of documcnl, with indication, where appropnate, of the relevant pa«ages

Relevant to claim No.

P,Y

WO. A, 95 22910 (PROCTER & GAMBLE) 31 August
1995

see claim 1

1-8

Form PCX ISA 210 (conitnuauon of second sheeij (July 1992

page 2 of 2

INTERNATIONAL SEARCH REPORT

Information on patent fanuly members

mationai Application No

PCT/US 95/01645

Patent document
cited in search report

Publication
date

Patenl family
member(s)

PublicsLtion
date

DE-A-1792760

30-05-74

AT-A-

293849

15-09-71

BE-A-

OCA

no 07

CH-A-

487597

31-03-70

DE-A-

1642142

22-04-71

FR-A-

ICC OOAO

23-05-69

GB-A-

1 1 nn /I c A

1199460

oo n7 in

NL-A-

DoOOObO

04-07-68

US-A-3681091

01-08-72

BE-A-

T CC7 Ad

/oo/4y

05-11-71

FR-A-

2096744

25-02-72

GB-A-

1313287

11-04-73

ib-t)4- / 1

AT-A-

293850

1 c no 7 1

BE-A-

708863

02-07-68

CH-A-

487596

"3 1 no 7r\
3i-U3-/U

FR-A-

1568002

23-05-69

GB-A-

1154079

04-06-69

NL-A-

6800059

utu/ oo

US-A-4748033

31-05-88

CA-A-

1316753

27-04-93

WO-A-9522910

31-08-95

US-A-
AU-B-

5431940
1924295

11-07-95
11-09-95

Form PCT ISA 210 Ipaient tamily anne>t July 1992;

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Full text of "USPTO Patents Application 10551504"

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